2. Referenced Documents
2.1 ASTM Standards: 2
D 1525 Test Method for Vicat Softening Temperature of
Plastics
E 473 Terminology Relating to Thermal Analysis
E 1142 Terminology Relating to Thermophysical Properties
E 1363 Test Method for Temperature Calibration of Thermomechanical Analyzers
E 2113 Test Method for Length Change Calibration of
Thermomechanical Analyzers
E 2206 Test Method for Force Calibration of Thermomechanical Analyzers
1. Scope
1.1 This test method is applicable to materials that soften
upon heating to a modulus less than 6.0 MPa. This test method
describes the determination of the temperature at which the
specific modulus of either 6.65 (Method A) or 33.3 MPa
(Method B) (equivalent to Test Method D 1525) of a test
specimen is realized by indentation measurement using a
thermomechanical analyzer as the test specimen is heated. This
temperature is identified as the indentation softening temperature. The test may be performed over the temperature range of
ambient to 300C.
NOTE 1This test method is intended to provide results similar to those
of Test Method D 1525 but is performed on a thermomechanical analyzer
using a smaller diameter indenting probe. Equivalence of results to those
obtained by Test Method D 1525 has been demonstrated on a limited
number of materials. Until the user demonstrates equivalence, the results
of this Test Method shall be considered to be independent and unrelated to
those of Test Method D 1525.
3. Terminology
3.1 DefinitionsSpecific technical terms used in this standard are defined in Terminologies E 473 and E 1142.
3.2 penetration softening temperature, [C], nthe temperature at which a test specimen has a modulus of either 6.65
or 33.3 MPa as measured in penetration.
1.2 This test method is not recommended for ethyl cellulose, poly (vinyl chloride), poly (vinylidene chloride) and other
materials having a large measurement imprecision (see Test
Method D 1525 and sections 5.3 and 14.1.2).
1.3 Electronic instrumentation or automated data analysis
and reduction systems or treatments equivalent to this test
method may be used.
NOTE 2Since all electronic data treatments are not equivalent, the
user shall verify equivalency to this test method.
(1)
where:
E = modulus, MPa,
F = force, N,
D = diameter of a circular, flat tipped probe, mm, and
d = penetration depth, mm.
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal
Analysis and Rheology Methods.
Current edition approved Feb. 1, 2004. Published March 2004.
2
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contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
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E 2347 04
1.0 mm in diameter, free of burrs and be perpendicular to the
axis of the probe. The tip shall protrude at least 0.1 mm from
the end of the probe.
6.1.3 Deflection Sensing Element, having a linear output
over a minimum range of 5 mm to measure the displacement of
the rigid penetration probe (see 6.1.2) to within 6 0.1 m.
6.1.4 Programmable Force Transducer, to generate a constant force (6 2.5 %) between 0.05 and 1.0 N that is applied to
the specimen through the rigid penetration probe (see 6.1.2).
6.1.5 Temperature Sensor, that can be positioned reproducibly in close proximity to the specimen to measure its temperature over the range of 25 to 300C to 6 0.1C.
6.1.6 Temperature Programmer and Furnace, capable of
temperature programming the test specimen from ambient to
300C at a linear rate of at least 2.0 6 0.2C/min.
6.1.7 Means of Providing a Specimen Environment, of inert
gas at a purge rate of 50 mL/min 6 5 %.
NOTE 5Typically, inert purge gas that inhibits specimen oxidation are
99.9+ % pure nitrogen, helium or argon. Dry gases are recommended for
all experiments unless the effect of moisture is part of the study.
6.1.8 Recording Device, to record and display the experimental parameters of penetration on the Y-axis (ordinate) to a
sensitivity of 6 0.1 m and of temperature on the X-axis
(abscissa) to a sensitivity of 6 0.1C.
6.2 Calipers, Micrometer, or other length measuring device
capable of a length measurement of up to 2 mm with a
precision of 6 1 m.
6. Apparatus
6.1 A thermomechanical analyzer consisting of:
6.1.1 Rigid Specimen Holder, of inert, low expansivity
material (< 1 m m-1 C-1) to center the specimen in the
furnace and to fix the specimen to mechanical ground.
6.1.2 Rigid Penetration Probe, of inert, low expansivity
material (< 1 m m-1 C-1) that contacts the specimen with an
applied compression force (see Fig. 1). The tip shall be 0.1 to
7. Hazards
7.1 Toxic or corrosive effluents, or both, may be released
when heating some materials and could be harmful to personnel and to apparatus.
E 2347 04
11.3.1 Set the value of Force (F) to 0.75 6 0.01 N.
11.3.2 Perform Scouting Experiment:
11.3.2.1 Using Eq 2 and an estimated value of do = 0,
estimate the deflection (d) to be used as the experimental
endpoint to three significant figures.
11.3.2.2 Center the test specimen on the stage with a surface
perpendicular to the loading nose of the penetration probe.
11.3.2.3 Load the penetration probe onto the center of the
test specimen with the force determined in 11.2.1 (Method A)
or 11.3.1 (Method B). Set the deflection signal to zero at
ambient temperature.
11.3.2.4 Heat the test specimen at 2.0 6 0.2C min-1 from
ambient temperature until the deflection d (determined in
11.3.3.1) is obtained while recording specimen deflection and
temperature. Once the deflection value is achieved, terminate
the temperature program and remove the load from the test
specimen. Cool the apparatus to ambient temperature.
11.3.2.5 Record the temperature at the deflection value d as
the estimated indentation softening temperature (T).
11.3.2.6 For ease of interpretation, record the thermal curve
with penetration displayed on the Y-axis and temperature on
the X-axis as illustrated in Fig. 2.
11.3.3 Determine the Baseline:
11.3.3.1 With no sample present, place the tip of the
penetration probe onto the center of the sample stage. Load the
probe with the force determined in 11.2.1 or 11.3.1. Set the
deflection scale signal to be zero at ambient temperature.
11.3.3.2 Heat the sample area at 2.0 6 0.2 C min-1 from
ambient temperature to a temperature 5C higher than T
determined in 11.3.3.3. Once the temperature program is
complete, remove the load from the probe and cool the
apparatus to ambient temperature.
11.3.3.3 Measure the deflection of the baseline at temperature T and record it as do.
E 2347 04
5 19.3 m
NOTE 6do is positive for a baseline that expands with temperature and
negative if the baseline contracts.
13. Report
12. Calculation
12.1 Calculate the deflection value as follows:
d 5 @3 F/4 D E# 2 do
(2)
where:
E = modulus, MPa,
F = force, N,
D = diameter of a circular, flat tipped probe, mm,
d = penetration depth, mm, and
do = baseline depth at temperature T, mm.
NOTE 7Note the identity Pa = N / m2
=
=
=
=
6.65 MPa,
0.15 N,
0.889 mm, and
0.0003 mm
15. Keywords
15.1 penetration temperature; softening; strain; stress; temperature; thermomechanical analysis (TMA); vicat temperature
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E 2347 04
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